The future of food testing which way to go?

Transcription

1 The future of food testing which way to go? Franz Ulberth European Commission, DG Joint Research Centre, Institute for Reference Materials and Measurements (IRMM)

2 The Joint Research Centre (JRC) European Commission s in-house science service Supporting EU policies with independent, evidence-based scientific and technical support ~ staff (2014) 6 locations 2

3 JRC's Mission As the Commission's in-house science service, the Joint Research Centre's mission is to provide EU policies with independent, evidencebased scientific and technical support throughout the whole policy cycle. Working in close cooperation with policy Directorates-General, the JRC addresses key societal challenges while stimulating innovation through developing new methods, tools and standards, and sharing its knowhow with the Member States, the scientific community and international partners. 3

4 Main competence areas Energy Clean transport Environment & Climate change Agriculture & Food security Health & Consumer protection Safety and security, including nuclear Information and communication technology 1 June

5 Source: Ercsey-Ravasz M, Toroczkai Z, Lakner Z, Baranyi J (2012) Complexity of the International Agro-Food Trade Network and Its Impact on Food Safety. PLoS ONE 7(5): e doi: /journal.pone , p.2. 5

6 Decision making 5-10 billion analytical data generated annually in EU costs of chemical measurements several tens of billion EURO p.a. in EU results only useful if comparable (to a limit, to other results, etc) irrespective of time or space

7 The lot is accepted if the analytical result of the laboratory sample does not exceed the respective maximum level taking into account the expanded measurement uncertainty

8 Compliance with regulatory limits and measurement uncertainty Result plus MU below limit Result below limit but limit within MU Result above limit but limit within MU Result minus MU above limit

9 1 June

10 Specific EU food safety legislation 10

11 EU food and feed legislation relating to methods of analysis Regulation (EC) No 882/2004 Preamble (17): Laboratories involved in the analysis of official samples should use methods of analysis that have, as far as possible, been validated. Article 11 (Methods of sampling and analysis): Para 1: Sampling and analysis methods used shall comply with relevant Community rules with internationally recognised rules or protocols, for example those CEN has accepted with other methods fit for the intended purpose Where para 1 does not apply, validation of methods of analysis may take place within a single laboratory according to an internationally accepted protocol

12 Standardised methods Easily available Complete documentation Proven performance Acceptance Consensus Market driven

13 Intergovernmental organisations Council Regulation (EC) No 491/2009 establishing a common organisation of agricultural markets and on specific provisions for certain agricultural products (Single CMO Regulation) "The methods of analysis for determining the composition of the products of the wine sector.shall be those recommended and published by the OIV." 1 June 2015 Commission Regulation (EEC) No 2568/91 of 11 July 1991 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis 13

14 International protocols for collaborative studies ISO 5725:1994 Parts 1-6 Accuracy (trueness and precision) of measurement methods and results IUPAC Protocol for the design, conduct and interpretation of method-performance studies AOAC OMA Appendix D: Guidelines for collaborative study procedures to validate characteristics of a method of analysis 1 June

15 Nested design Level (j=1,2, q) q Lab (i=1,2, p) p1 p2 Run (n) n1 n2 n1 n2 1 June

16 Select method Peer-verification Optimise method In-house method characterisation Range LOD/LOQ Precision Trueness Ruggedness Test item preparation and testing Homogeneity Stability Collaborative study Pre-trial Main-trial Collaborative study workflow NO Desired performance characteristics YES NO Desired performance characteristics YES Publish method 1 June

17 Criteria approach Mandating a certain analytical method in regulations denies the analyst to choose the most appropriate method for a given task discourages development of alternative approaches and the use of automation complicates administrative procedures if the prescribed method needs to be replaced by a more suitable one

18 Paradigm shift Method selection based on procedure Method selection based on performance Fit-for-purpose

19 Commission Regulation (EC) No 333/2007

20 EURL PAH proficiency test 1 June

21 EURL PAH proficiency test 1 June

22 Collaborative study results Sample EXWFLOUR FISH_B IF_2010 IF_2011 MEAT_A Number of laboratories Number of laboratories considered as non compliant Number of outliers (laboratories) Number of accepted results Mean value, x, μg/kg Bias ( ) n.a. n.a. n.a. n.a. n.a. 1 June 2015 <2*u (see Equation 3) n.a. n.a. n.a. n.a. n.a. Repeatability standard deviation s r, μg/kg Repeatability relative standard deviation, RSD r, % Repeatability limit r [r = 2,8 s r ], μg/kg Reproducibility standard deviation s R, μg/kg Reproducibility relative standard deviation, RSD R, % Reproducibility limit R [R = 2,8 s R ], μg/kg Recovery, % HorRat value

23 Modular validation Physical sample preparation Sub-sampling Extraction Clean-up (Derivatisation). Measurement 1 June

24 Practical approaches In-house validation Designed experiments First uncertainty estimate Use method Better uncertainty estimate PT schemes QA results CRMs R. Macarthur

25 Life cycle of analytical method Proficiency test Validated method Internal Quality Control Verify implementation

26 Equivalence of methods 1 June

27 Uncertainty components Heterogeneity + Sampling Uncertainty + Analytical Uncertainty Measurement Uncertainty Decision Uncertainty Nordtest

28 Sources of uncertainty Sampling Heterogeneity Sampling strategy (e.g. random, stratified random, proportional etc.) Effects of movement of bulk medium (particularly density or size selection) Physical state of bulk (solid, liquid, gas) Temperature and pressure Effect of sampling process on composition (e.g. differential adsorption in sampling system). Contamination Transportation and preservation of sample Homogenisation and/or sub-sampling effects Drying Milling Dissolution Extraction Contamination Derivatisation (chemical effects) Dilution errors (Pre-)Concentration Control of speciation effects. Nordtest

29 Examples Measurement uncertainty Sampling Analytical Total Nitrate in lettuce 14.5 % 7.6 % 16.4 % Retinol in baby food Aflatoxins in pistachio nuts 9.9 % 16.6 % 19.4 % 45.2 % 54.2 % 70.5 %

30 Way forward for regulators Acceptance sampling as being indicated by the Codex Alimentarius General Guidelines on Sampling (variability of acceptance sampling plans!) Uncertainty of sampling approach (magnitude of sampling uncertainty!) Define sampling procedure and ignore what the actual variability is (pragmatic approach!)

31 Joint Research Centre (JRC) Robust science for policy making Web: ec.europa.eu/jrc Contact: